EP2796192A2 - Stirrer cell module and method of using - Google Patents

Stirrer cell module and method of using Download PDF

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Publication number
EP2796192A2
EP2796192A2 EP14163593.8A EP14163593A EP2796192A2 EP 2796192 A2 EP2796192 A2 EP 2796192A2 EP 14163593 A EP14163593 A EP 14163593A EP 2796192 A2 EP2796192 A2 EP 2796192A2
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EP
European Patent Office
Prior art keywords
stirrer
baffle
cell module
central passage
membrane
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP14163593.8A
Other languages
German (de)
English (en)
French (fr)
Inventor
Jason S. Pellegrino
Lixiang Xiao
Richard Morris
James J. Hathcock
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pall Corp
Original Assignee
Pall Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Pall Corp filed Critical Pall Corp
Publication of EP2796192A2 publication Critical patent/EP2796192A2/en
Withdrawn legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/86—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis co-operating with deflectors or baffles fixed to the receptacle
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M99/00—Subject matter not provided for in other groups of this subclass
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/082—Investigating permeability by forcing a fluid through a sample
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2315/00—Details relating to the membrane module operation
    • B01D2315/10—Cross-flow filtration
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules

Definitions

  • membranes are evaluated to provide a desired balance between selectivity and flux.
  • Stirrer cell modules are used in small scale manufacturing and research, e.g., to preliminarily evaluate membrane candidates for use in desired applications and devices.
  • the module is in the form of a stirred tank and a membrane is fitted in the bottom.
  • a feed or challenge fluid is introduced into the module, the module is operated, and the flux versus the selectivity is analyzed for each membrane.
  • membranes may be further evaluated, e.g., they can be scaled up and tested using cross-flow or trans-membrane pressure (TMP) conditions, for example, using a tangential flow filtration (TFF) cassette or holder.
  • TMP trans-membrane pressure
  • stirrer cell module that can be operated to provide efficient membrane testing.
  • the stirrer cell module comprises (a) a bottom wall including a port; (b) a body comprising an inner wall; (c) a rotatable stirrer comprising a shaft and at least one member projecting from the shaft; and, (d) a baffle comprising an upper surface, a lower surface, at least a central passage, the central passage passing through both the upper and lower surfaces, and a side comprising an outer surface, the outer surface contacting the inner wall of the body, wherein the stirrer shaft passes through the central passage of the baffle and the stirrer member is arranged between the bottom wall and the lower surface of the baffle.
  • the central passage comprises a passage with a tapered side wall.
  • the baffle can further comprise a plurality of flow passages passing through both the upper and lower surfaces, and the flow passages can comprise perforations and/or fins.
  • stirrer cell module comprises (a) a bottom wall including a port; (b) a body comprising an inner wall; (c) a rotatable stirrer comprising a shaft and at least one member projecting from the shaft; and, (d) a baffle comprising an upper surface, a lower surface, a central passage, a plurality of fluid flow passages, the central passage and the plurality of fluid flow passages passing through both the upper and lower surfaces, and a side comprising an outer surface, the outer surface contacting the inner wall of the body, wherein the stirrer shaft passes through the central passage of the baffle and the stirrer member is arranged between the bottom wall and the lower surface of the baffle.
  • the fluid flow passages of the baffle comprise perforations and/or fins.
  • a method of using a stirrer cell module is provided.
  • Another embodiment of the invention provides a baffle for use in a stirrer cell module.
  • a stirrer cell module comprises (a) a bottom wall including a port; (b) a body comprising an inner wall; (c) a rotatable stirrer comprising a shaft and at least one member (typically fixed to the shaft) and projecting from the shaft; and, (d) a baffle comprising an upper surface, a lower surface, at least a central passage, the central passage passing through both the upper and lower surfaces, and a side comprising an outer surface, the outer surface contacting the inner wall of the body, wherein the stirrer shaft passes through the central passage of the baffle and the stirrer member is arranged between the bottom wall and the lower surface of the baffle.
  • the baffle can further comprise a plurality of flow passages passing through both the upper and lower surfaces, and the flow passages can comprise perforations and/or fins.
  • stirrer cell module comprises (a) a bottom wall including a port; (b) a body comprising an inner wall; (c) a rotatable stirrer comprising a shaft and at least one member projecting from the shaft; and, (d) a baffle comprising an upper surface, a lower surface, a central passage, a plurality of fluid flow passages, the central passage and the plurality of fluid flow passages passing through both the upper and lower surfaces, and a side comprising an outer surface, the outer surface contacting the inner wall of the body, wherein the stirrer shaft passes through the central passage of the baffle and the stirrer member is arranged between the bottom wall and the lower surface of the baffle.
  • the fluid flow passages of the baffle comprise perforations and/or fins.
  • the central passage of the baffle comprises a passage with a tapered side wall.
  • the baffle comprises a central hub and a plurality of fins attached to the hub.
  • the central hub has an axis, and the fins are inclined relative to the axis of the central hub.
  • the baffle comprises at least 3 fins.
  • an embodiment of the method comprises introducing a fluid into an embodiment of the stirrer cell module, wherein the stirrer cell module includes a membrane therein, operating the stirrer, obtaining a filtrate passing through the membrane, and analyzing flux versus selectivity for the membrane.
  • a method for operating a stirrer cell module comprises a bottom wall including a port; a body comprising an inner wall; a rotatable stirrer comprising a shaft and at least one member projecting from the shaft; a baffle comprising an upper surface, a lower surface, a central passage, the central passage passing through both the upper and lower surfaces, and a side comprising an outer surface, the outer surface contacting the inner wall of the body; and, a membrane having an upstream surface and a downstream surface, the downstream surface contacting the bottom wall, wherein the stirrer shaft passes through the central passage of the baffle and the stirrer member is arranged between the bottom wall and the lower surface of the baffle; the method comprising introducing fluid into the body, rotating the stirrer, and passing fluid through the through the membrane and through the port in the bottom wall.
  • the method further comprises analyzing flux versus selectivity for the membrane.
  • a baffle for use in a stirrer cell module, the baffle comprising a central passage, an upper surface, a lower surface, and an outer surface, wherein the central passage pass through both the upper and lower surfaces.
  • the central passage comprises a passage with tapered side walls.
  • the baffle can further comprise a plurality of flow passages passing through both the upper and lower surfaces, and the flow passages can comprise perforations and/or fins.
  • embodiments of baffles according to the invention are suitable for use in existing stirrer cell modules, e.g., the modules can be "retrofit" with the baffles.
  • the baffle comprising a central passage, fluid flow passages, an upper surface, a lower surface, and an outer surface, wherein the central and fluid flow passages pass through both the upper and lower surfaces.
  • the fluid flow passages comprise perforations and/or fins.
  • baffles and stirrer cell modules including baffles
  • the baffle can be effectively operated. Without being limited to any particular mechanism, it is believed that the baffle impedes the momentum transfer towards the upper fluid layers, enabling stirring at higher revolutions per minute and higher flux. It is also believed that by preventing momentum transfer away from the membrane surface, the baffle traps the kinetic energy (turbulence/pressure) imparted by the stirrer near the surface of the membrane, which enhances the transport of the retained solute away from the active filtration site and reduces concentration polarization. It is believed that this permits higher transmembrane flux conditions that are more representative of tangential flow filtration (TFF), without the artifacts that might otherwise be introduced by high flux conditions without the enhanced mixing.
  • TMF tangential flow filtration
  • Additional advantages include the requirement for less challenge solution (e.g., the need for additional challenge solution is reduced or eliminated), reduced testing time and cost. Alternatively, or additionally, testing is carried out more efficiently, e.g., the results are more predictive, resulting in weeding out less desirable membrane candidates before subsequent scale up testing, further reducing the overall test time and cost.
  • the use of baffles reduces vortex formation.
  • a baffle 100 comprises a central passage 150, an upper surface 110, a lower surface 120, and a side 130 comprising an outer surface 131, wherein the central passage passes through both the upper and lower surfaces.
  • the baffle 100 further comprises a plurality of fluid flow passages 160, wherein the fluid flow passages pass through both the upper and lower surfaces of the baffle. In some embodiments, it is believed that the flow passages allow for drainage and reduced air entrapment.
  • the illustrated baffle includes axially arranged fins 175, fluid flow passages 160 comprising non-spherical openings, a central hub 180 having an axis 185, and an outer ring 135 including the outer surface 131, wherein the fins are interposed between, and connected to, the central hub and the outer ring.
  • the fins are preferably inclined relative to the axis of the central hub, and comprise a first edge 175A and a second edge 175B. In some embodiments (not shown), the fins include a curve between the first and second edges.
  • the illustrated baffle 100 includes fluid flow passages 160 comprising spherical holes or perforations 190.
  • baffle configurations are suitable for use in the invention.
  • the fluid flow passages 160 comprise spherical or generally spherical openings (e.g., perforations 190), as shown in Figure 3 , for example, the central passage 150 (for a stirrer shaft) has a larger inner diameter than the individual diameters of the fluid flow passages 160.
  • the fluid flow passages can have similar or identical inner diameters or open areas compared to each other, or they can be varied.
  • the outer surface 131 of the baffles are continuous, having outer diameters providing an interference fit with the inner wall of the body of the stirrer cell module.
  • portions of the outer surface 131 can be cut away, for example, as shown in Figures 3 and 6 (e.g., providing a non-continuous outer surface 131A), providing fluid flow passages, while still providing an interference fit with the inner wall of the body of the stirrer cell module.
  • the central passage 150 can have any suitable configuration such as shape and size (e.g., diameter).
  • the central passage can have a tapered side wall (e.g., as shown in Figure 1A ), or a non-tapered (e. g., straight) side wall (e. g., as shown in Figures 1B , 2A-2C , and 3 ).
  • the side wall is preferably tapered from both the upper and lower surfaces, e.g., as shown in Figure 1A , but can be tapered from only the upper or the lower surface.
  • the central passage has a diameter in the range of from about 5 mm to about 30 mm, preferably, the central passage has a diameter of about 25 mm or less. However, the central passage can have a larger or small diameter.
  • the passage can have a non-spherical opening, e.g., a triangular, rectangular, square, or other shape opening.
  • the opening can have a continuous inner surface 151 (e.g., as shown in Figures 1A-1B , 2 , 4 , and 5 ) or an inner surface that is cut away (e.g., providing a non-continuous inner surface 151A, as shown in Figures 3 and 6 ).
  • a stirrer cell module 1000 comprises a pressure-sealed cover 700, a fluid inlet/outlet port 710, at least one vent 701 (an optional second vent 701 is illustrated), a gas inlet port 702 (for pressurizing the module), a membrane holder 600 comprising a bottom wall 601 including a permeate outlet port 601A, a body 500 comprising a central lumen and including an inner wall 501 and an outer wall 502, a baffle 100 including a central passage 150, an upper surface 110 and a lower surface 120, the central passage passing through both the upper and lower surfaces, the baffle also comprising a side 130 comprising an outer surface 131 in contact with the inner wall 501 of the body 500.
  • the baffle 100 further comprises fluid flow passages 160, wherein the fluid flow passages pass through both the upper and lower surfaces
  • the illustrated stirrer cell module also comprises a stirrer 400, comprising a shaft 410 and an impeller 420 (in the illustrated embodiment, comprising two projecting members or arms 421A, 42 1 B, extending outwardly from the shaft), wherein the shaft passes through the center hole of the baffle and the impeller is located between the lower surface of the baffle and the bottom wall (e.g., as also shown in Figure 7 ).
  • the module includes a moveable support 900 (shown in more detail in Figure 5A ), sealably engaging the membrane holder with the body.
  • the support 900 is lowered, a membrane will be placed on the bottom wall 601 of the membrane holder 600, and the support is raised, sealably engaging the membrane holder with the body.
  • the module can include additional components, for example, a means for rotating the stirrer such as a magnet or motor 950, one or more bearings (e.g., associated with the motor and/or stirrer), one or more o-rings and/or gaskets, and/or one or more tube fittings and/or ports and/or valves (e.g., for gas pressurization, venting/pressure relief, and permeate).
  • a means for rotating the stirrer such as a magnet or motor 950, one or more bearings (e.g., associated with the motor and/or stirrer), one or more o-rings and/or gaskets, and/or one or more tube fittings and/or ports and/or valves (e.g., for gas pressurization, venting/pressure relief, and permeate).
  • Stirrer cell modules according to embodiments of the invention can have any suitable capacity, e.g., several milliliters (mL) or more. In some embodiments, the modules have a capacity of several hundred mL, or several thousand mL, or more. Typically, stirrer cell modules according to embodiments of the invention have capacities of about 3 mL to about 600 mL, or more.
  • a variety of body configurations are suitable for use in the invention, and such elements and configurations can be commercially available.
  • the lower end 430 of the stirrer 400 has a generally "T-shaped" appearance, e.g., wherein the stirrer shaft 410 has a vertical axis and the impeller 420 has two members or arms 421a, 421b projecting perpendicular or substantially perpendicular to the vertical axis, and the center of the impeller is mounted to the lower end of the shaft, but the invention is not so limited.
  • the impeller can have three or more arms and/or bent arms and/or the member(s) can project non-parallel or parallel to the vertical axis of the shaft.
  • the impeller can be mounted to the shaft at a distance from the lower end of the shaft.
  • the baffle, body, membrane holder, support, cover, and stirrer can be fabricated from any suitable rigid impervious material, including any impervious thermoplastic material, which is compatible with the fluid(s) being used.
  • the baffle, body, membrane holder, and cover can be fabricated from a polymer, or a metal, such as stainless steel.
  • the surfaces contacting the stirredr fluids are non-metal for those embodiments wherein solvent resistance is less of a concern, and the surfaces contacting the stirred fluids are metal (e.g., stainless steel) and/or glass (e.g., borosilicate glass) wherein solvent resistance is of interest.
  • the shaft and impeller are coated with PTFE.
  • the body and the baffle are each fabricated from a polymer; in some embodiments, the body is a transparent or translucent polymer, such as an acrylic, polypropylene, polystyrene, sulfone, or a polycarbonated resin.
  • a transparent or translucent polymer can be desirable for viewing the contents of the module while the module is operating.
  • the membranes can have any suitable pore structure, e.g., a pore size (for example, as evidenced by bubble point, or by K L as described in, for example, U.S. Patent 4,340,479 , or evidenced by capillary condensation flow porometry), a mean flow pore (MFP) size (e.g., when characterized using a porometer, for example, a Porvair Porometer (Porvair plc, Norfolk, UK), or a porometer available under the trademark POROLUX (Porometer.com; Belgium)), a pore rating, a pore diameter (e.g., when characterized using the modified OSU F2 test as described in, for example, U.S. Patent 4,925,572 ), or a removal rating.
  • a pore size for example, as evidenced by bubble point, or by K L as described in, for example, U.S. Patent 4,340,479 , or evidenced by capillary condensation flow porometry
  • MFP mean flow pore
  • the membranes can have any suitable diameter and effective membrane area.
  • the membranes have diameters of at least about 25 mm and effective membrane areas of at least about 0.9 cm 2 , more typically, effective membrane areas of at least about 3.5 cm 2 .
  • Other illustrative membrane diameters and effective membrane areas are at least about 45 mm and at least about 11.5 cm 2 ; at least about 64 mm and at least about 27.0 cm 2 ; at least about 76 mm and at least about 38.5 cm 2 ; at least about 90 mm and at least about 54.5 cm 2 ; at least about 150 mm and at least about 162 cm 2 , or more.
  • a tapered solid plastic disc baffle with an 8.9mm central hole (as generally illustrated in Figure 1A ) is installed into the stirrer cell module using force fit, locating the baffle about 1 cm over the upstream surface of the membrane, wherein the baffle can be removed for the direct comparison of the baffle's effect.
  • the module has a capacity of about 50 mL.
  • the membranes tested in the module (using a dextran challenge) are about 44.5 mm in diameter and have effective membrane areas of about 13.4 cm 2 . Identical grades of membranes are placed in each container and tested.
  • the stirrer cell module is operated while regulating a constant permeate flux.
  • the stirrer cell is pressurized to 20 psi with nitrogen and the magnetic stirrer rotated at 1600 RPM using a VWR digital stir plate.
  • the permeate flow is set to 70 liters per square meter per hour (LMH) using a Rainin Precision Peristaltic Pump (Mettler Toledo; Columbus, OH) downstream of the cell modules.
  • a stirrer cell module including a baffle is set up and operated as generally described in Example 1, with the exception that the stirrer is rotated at 1000 RPM, and the constant permeate flux is 25 LMH.
  • the R90 is 17 kDa.
  • a TFF cassette test using the same membrane grade and dextran mix provides an R90 of 16-18 kDa.
  • this example demonstrates that using a stirrer cell module including a baffle according to an embodiment of the invention (using different stirring rates and permeate fluxes) provides mixed dextran R90 results more representative of TFF cassette performance than those the results obtained using a stirrer cell module without the baffle.
  • This example demonstrates the reduction in vortex formation using a cell stirrer module including baffles with different diameter central passages.
  • Stirrer cell modules including baffles as generally shown in Figures 1B and 4 are set up.
  • stirrer cell modules without baffles are also set up for each set of experiments.
  • a 44.5 mm module is used, and the baffles have central diameters of 8.9 mm, 10.2 mm, 11.4 mm, 12.7 mm, and 19.1 mm.
  • the baffles are plastic plates wedged against the inner wall of a polysulfone cylindrical body.
  • the baffle is located about 1 cm above the surface of the membrane holder.
  • Challenge solution is introduced and the module is pressurized with nitrogen gas at 5 psi (34.5 kPa).
  • the stirrer RPM is confirmed by a stroboscope. Pictures are taken of the vortex heights at different stir speeds, and the vortex heights from the pictures are analyzed using Micrometrics Image Analysis Software by calibrating each image to a reference length.
  • baffles In another set of experiments, a 63.5 mm module is used, and the baffles have central diameters of 8.9 mm, 12.7 mm, and 19.1 mm.
  • the example shows that the vortex can be reduced using baffles with central passages, and a variety of central diameters are suitable.
  • This example demonstrates the reduction in vortex formation using a cell stirrer module including baffles with different thicknesses and different numbers of fins.
  • Stirrer cell modules including baffles as generally shown in Figures 2 and 5 are set up.
  • a stirrer cell module without baffles is also set up.
  • a 44.5 mm module is used, and two sets of baffles are used, one set has a thickness of 3.4 mm and 3, 6, and 10 blades, the other set has a thickness of 6.4 mm and 3, 6, and 10 blades.
  • the baffles are plastic plates wedged against the inner wall of a polysulfone cylindrical body.
  • the baffle is located about 1 cm above the surface of the membrane holder.
  • Challenge solution is introduced and the module is pressurized with nitrogen gas at 5 psi (34.5 kPa).
  • the stirrer is rotated at 0, 240, 600, 800 and 1000 RPM.
  • the example shows that the vortex can be reduced using a baffle with fins, and a variety of number of blades and baffle thicknesses are suitable.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Apparatus Associated With Microorganisms And Enzymes (AREA)
EP14163593.8A 2013-04-26 2014-04-04 Stirrer cell module and method of using Withdrawn EP2796192A2 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US13/871,160 US20140318230A1 (en) 2013-04-26 2013-04-26 Stirrer cell module and method of using

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EP2796192A2 true EP2796192A2 (en) 2014-10-29

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EP14163593.8A Withdrawn EP2796192A2 (en) 2013-04-26 2014-04-04 Stirrer cell module and method of using

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US (1) US20140318230A1 (enrdf_load_stackoverflow)
EP (1) EP2796192A2 (enrdf_load_stackoverflow)
JP (1) JP2014223613A (enrdf_load_stackoverflow)
KR (1) KR20140128245A (enrdf_load_stackoverflow)
CN (1) CN104117286A (enrdf_load_stackoverflow)
IN (1) IN2014DE01009A (enrdf_load_stackoverflow)
SG (1) SG10201401303QA (enrdf_load_stackoverflow)

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CN111249941B (zh) * 2020-02-10 2021-09-14 深圳市尚水智能设备有限公司 一种用于固体在液体中分散的叶轮组件及使用该组件的固液混合设备

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CN104117286A (zh) 2014-10-29
IN2014DE01009A (enrdf_load_stackoverflow) 2015-06-05
JP2014223613A (ja) 2014-12-04

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